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Method for purifying northeast cyrtominetin from plant rhizoma dryopteris crassirhizomae

A technology of Northeast Guanzhongsu and Mianma Guanzhong, which is applied in the direction of fern/filamentous plant medical raw materials, drug combinations, anti-tumor drugs, etc., can solve the problems of difficult operation, poor water solubility of Northeast Guanzhongsu, large Porous resin separation is difficult and other problems, to achieve the effect of less reagent loss and good impurity removal effect

Inactive Publication Date: 2010-06-16
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Wang Haining et al. optimized the macroporous resin suitable for separating Mianmaguanzhong Zhongdongguanzhongsu as DM130, and studied the process conditions and parameters of the optimized macroporous resin for separating Mianmaguanzhong, but Dongbeiguanzhongsu Poor water solubility, difficult to separate macroporous resin, difficult to operate

Method used

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  • Method for purifying northeast cyrtominetin from plant rhizoma dryopteris crassirhizomae

Examples

Experimental program
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Effect test

Embodiment 1

[0036] Take Mianmaguanzhong medicinal materials, crush them, put 10kg into the extraction tank, add 70L of 90% ethanol and 20g of calcium hydroxide, stir and heat to 50°C, extract twice, each time for 2 hours, combine the extracts and filter, adjust the pH to 5. Recover under reduced pressure to an ethanol concentration of 40%, let it stand for 12 hours, and filter out 1 kg of precipitate. Dissolve under reflux in chloroform and add 2% 767 injection of activated carbon to decolorize for 2 hours, filter, add to 20kg of silica gel, recover chloroform, dry and install a short and thick column, first wash impurities with 120L methanol, and then elute the fraction with ethyl acetate, thin layer Detection, collect the fractions and recover to 1 / 10 of the original volume, place the crystals, filter out the crystals, reflux with acetone to saturate and dissolve, cool and stand for crystallization, filter out the crystals and redissolve and crystallize once, and dry at low temperature t...

Embodiment 2

[0038] Take Mianmaguanzhong medicinal materials, crush them, put 10kg into the extraction tank, add 70L of 90% ethanol and 10g of calcium hydroxide, stir and heat to 75°C, extract twice, each time for 2 hours, combine the extracts and filter, adjust the pH to 7. Recover under reduced pressure to an ethanol concentration of 30%, let it stand for 8 hours, and filter out 1.1 kg of precipitate. Dissolve under reflux in chloroform and add 1% 767 injection of activated carbon for decolorization for 1 hour, filter, add to 18kg of silica gel, recover chloroform, dry it and put it into a short and thick column, first wash the impurities with 72L methanol, then elute the fraction with ethyl acetate, thin layer Detection, collecting the fractions and recovering them to 1 / 15 of the original volume, placing the crystals on place, filtering out the crystals in acetone, refluxing to saturate and dissolving, cooling and standing for crystallization, filtering out the crystals and redissolving ...

Embodiment 3

[0040] Take Mianmaguanzhong medicinal materials, crush them, put 10kg into the extraction tank, add 50L of 80% ethanol and 20g of calcium hydroxide, stir and heat to 60°C, extract three times, each time for 1.5 hours, combine the extracts and filter, adjust the pH to 6 with sulfuric acid , recovered under reduced pressure to an ethanol concentration of 50%, left for 10 hours, and 1.1 kg of precipitate was filtered out. Dissolve under reflux in chloroform and add 1.5% 767 injection of activated carbon for decolorization for 2 hours, filter, add to 19kg of silica gel, recover chloroform, install short and thick column after drying, first wash impurities with 100L methanol, and then elute the fraction with ethyl acetate, thin layer Detection, collect the fractions and recover to 1 / 8 of the original volume, place the crystals, filter out the crystals, reflux and saturate with acetone to dissolve, cool and stand for crystallization, filter out the crystals, redissolve and crystalliz...

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Abstract

The invention relates to a method for purifying northeast cyrtominetin from plant rhizoma dryopteris crassirhizomae, comprising the following steps of: using the rhizoma dryopteris crassirhizomae as raw materials, extracting by using alcohol-alkali, adjusting acid, concentrating and crystallizing, dissolving chloroform, decoloring active carbon, separating silicagel column, dissolving and recrystallizing acetone. The process has easy operation, high purity of the product and low cost; and all organic solvents can be utilized repeatedly after recycling.

Description

Technical field: [0001] The present invention relates to a method for purifying the Northeast Rhododendron from the plant S. chinensis, and adopts the processes of organic solvent extraction, active carbon decolorization, silica gel column separation and purification to prepare the Northeast Rhizoma. Background technique: [0002] Northeast Guanzhongsu, also known as Mianma Guanzhongsu, is a tetracyclic phloroglucinol derivative. [0003] English name: Dryocrassin; [0004] Molecular formula: C 43 h 48 o 16 ; [0005] Molecular weight: 820.83; [0006] Molecular formula: [0007] [0008] Physical properties: yellow crystal (acetone), melting point 201-203°C (also reported 207-214°C, 215-218°C); hardly soluble in water, soluble in benzene, ether, carbon tetrachloride, pentanol, acetone , Most organic solvents such as glacial acetic acid and alkaline aqueous solution. [0009] Dongbei Guanzhongsu is the main active ingredient in the antimalarial activity and antitu...

Claims

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Application Information

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IPC IPC(8): A61K36/11A61P35/00A61P33/06A61P33/12A61K125/00A61K135/00
Inventor 刘东锋郭琴杨成东
Owner NANJING ZELANG MEDICAL TECH
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